反应详情

4-Chlorobutyrophenone (1.8 g) and thiourea (0.8 g) is dissolved in ethanol (50 ml) and the solution is refluxed for 2 hours. To the mixture are added 1-methyl-5-chloro-1,2,3,4-tetrazole (1.2 g) and 10% aqueous sodium hydroxide (5 ml) and the mixture is further refluxed for 3 hours. Ethanol is distilled off and water is added to the residue. The mixture is extracted with chloroform. The chloroform solution is washed with water and saturated aqueous sodium chloride and dried over magnesium sulfate. Chloroform is distilled off. The residue is purified by column chromatography (Wakogel C-200, eluatn: chloroform) and the product is recrystallized from methanol-water to obtain 1-methyl-5-(3-benzoylpropyl)thio-1,2,3,4-tetrazole (0.3 g) as colorless needles, m.p. 57.5°-58° C.

1. temperaturethe solution is refluxed for 2 hours
2. temperaturethe mixture is further refluxed for 3 hours
3. distillationEthanol is distilled off
4. additionwater is added to the residue
5. extractionThe mixture is extracted with chloroform
6. washThe chloroform solution is washed with water and saturated aqueous sodium chloride
7. dry with materialdried over magnesium sulfate
8. distillationChloroform is distilled off
9. customThe residue is purified by column chromatography (Wakogel C-200, eluatn: chloroform)
10. customthe product is recrystallized from methanol-water